CN105195231A - Preparation method for after-treatment hydrocracking catalyst - Google Patents
Preparation method for after-treatment hydrocracking catalyst Download PDFInfo
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Abstract
The invention discloses a preparation method for an after-treatment hydrocracking catalyst. The method includes the steps that 1, a hydrocracking catalyst carrier is prepared; 2, the catalyst carrier is steeped in steeping liquid containing active metal components and then dried and calcined at low temperature; 3, after matter capable of changing the arrangement of active metals is dissolved in a solvent according to a certain proportion, the catalyst obtained from the step 2 is steeped in the mixture; 4, materials obtained from the step 3 are dried and calcined for 1-10 hours at the low temperature of 150-400 DEG C, and the final after-treatment hydrocracking catalyst is obtained. The matter capable of changing the arrangement of the active metals is one or more of a phosphoric acid complexing agent, an alcohol amine complexing agent, an aminocarboxylic acid complexing agent, a hydroxy carboxylic acid complexing agent, an organic phosphonic acid complexing agent and a polyacrylic acid complexing agent. The after-treatment hydrocracking catalyst prepared through the method is higher in hydrogenation activity and hydrogenation selectivity, higher in selectivity for middle distillate, and suitable for treating the hydrocracking catalysts composed of various different metals.
Description
Technical field
The present invention relates to catalysis technical field, be specially a kind of preparation method of post processing type hydrocracking catalyst, especially high aromatic hydrocarbons heavier hydrocarbon feeds is processed, and the distribution of hydrogenation active component in hydrocracking catalyst and existence form can be regulated, and then improve the method for hydrocracking catalyst activity.
Background technology
Hydrocracking technology, as solving the gentle major programme of separating environment stress problems of crude quality variation, is more and more subject to the attention of Petrochemical Enterprises.The core of hydrocracking is hydrocracking catalyst, and hydrocracking catalyst is a kind of bifunctional catalyst, and it is simultaneously containing acidic components and hydrogenation component.Hydrogenation activity is generally selected from VI B race in the periodic table of elements and group VIII metal provides; And the source of acidity comprises the carrier such as zeolite and inorganic oxide, the carrier of hydrocracking catalyst also needs to provide specific surface and pore volume to carry hydrogenation metal and reaction compartment simultaneously.Due in the catalyst adopting conventional method to prepare, the dispersion of active component in the different aluminium oxide of pore structure and molecular sieve is uncontrollable, cause more active component to be dispersed in can not touch in the interval of reactant, cause the great waste of active metal.And the active component in catalyst is after high-temperature roasting, can produce comparatively noticeable effort with carrier, form low activity component, cause active component not easily sulfuration in catalyst, hydrogenation activity is low.Finally cause hydrocracking catalyst hydrogenation component inharmonious with coordinating of Cracking Component, hydrogenation cracking activity is low.Along with the quickening of crude oil heaviness, in poor quality, the technology finding suitable control hydrocracking reaction activity is very urgent.
CN201119819.2 discloses a kind of preparation method of petroleum hydrocarbon hydrocracking catalyst, comprises and catalyst carrier being shaped, then carry out post processing with ammonium salt-containing and aqueous acid.Adopt this kind of method to carry out post processing to hydrocracking catalyst and mainly modulation is carried out to the Acidity of catalyst, modulation can not be carried out to the hydrogenation active component of catalyst.And the stability of this type of post-processing catalyst needs to be improved further.
CN201110133725.4 discloses a kind of special-shaped hydrocracking catalyst and its preparation method and application, method for preparing catalyst adopts the method for post-treatment solution, make metal uniform deposition on carrier, and do not move in follow-up dry run, reach metal dispersion even.Metal dispersion can be made even, and make carrier and metal have good coordinating, be that catalytic performance improves.This invention hydrocracking catalyst optimum is used for middle oil type hydrocracking process.The method is mainly in order to make active metal reach dispersed, but homodisperse active metal can not reach the higher accumulation number of plies, has bigger difference with the highly active hydrogenation sites of formation.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of method of hydrocracking catalyst being carried out to post processing.The method can according to the pore structure of the heterogeneity of oil product and molecular sieve and other porous masses, active component is distributed again, and by regulating the difference selecting material, and add the mol ratio of material and hydrogenation active component, control the form of active component.Make different hydrocracking catalysts be suitable for processing variant oil product, be particularly suitable for processing high aromatic hydrocarbons hydrocarbon material inferior.
The present invention is that a kind of preparation method of post processing type hydrocracking catalyst comprises the following steps:
1) carrier of hydrocracking catalyst is prepared;
2) adopt equi-volume impregnating to be impregnated in catalyst carrier the maceration extract containing active metal component, then dry, at 200 ~ 400 DEG C low-temperature bake 1 ~ 10 hour.
3) step 2 is impregnated into after the material that can change active metal arrangement is by a certain percentage dissolved in solvent) catalyst that obtains;
4) step 3) material that obtains carries out drying, be within 1 ~ 10 hour, obtain final post processing type hydrocracking catalyst 150 ~ 400 DEG C of low-temperature bake times;
Wherein, step 3) described in the material that can change active metal arrangement be one or more in phosphoric acid class, alcamines, aminocarboxylic acids, hydroxycarboxylic acid, organic phosphine acids, polyacrylic complexing agent;
The described material addition that can change active metal arrangement is 0.1 ~ 5 with the mol ratio of active metal component in catalyst, preferably 0.1 ~ 3.
In the preparation method of post processing type hydrocracking catalyst of the present invention, step 2) described in low-temperature bake condition be preferably: roasting 1 ~ 3 hour at 300 ~ 400 DEG C.
In the preparation method of post processing type hydrocracking catalyst of the present invention, described phosphoric acid class is one or more in tripolyphosphate, pyrophosphoric acid and hexa metaphosphoric acid; Alcamines is one or more in MEA, diethanol amine and triethanolamine; Aminocarboxylic acids is one or more in nitrilotriacetic acid (NTA), ethylenediamine tetra-acetic acid (EDTA), diethylenetriamine pentacarboxylic acid (DTPA); Hydroxycarboxylic acid is one or more in tartaric acid, heptonic acid, gluconic acid, alginic acid; Organic phosphine acids is one or more in ATMP (ATMP), HEDP (HEDPA), ethylenediamine tetraacetic methene phosphoric acid (EDTMPA), diethylene triamine pentamethylene phosphonic (DETPMPA) and amine three methene phosphoric acid; Polyacrylic is one or more in HPMA (HPMA), polyacrylic acid (PAA), poly-hydroxy acrylic acid, maleic acrylic copolymer and polyacrylamide.
In the preparation method of post processing type hydrocracking catalyst of the present invention, the described material that can change active metal arrangement is hydroxycarboxylic acid complexing agent or organic phosphine acids complexing agent.
In the preparation method of post processing type hydrocracking catalyst of the present invention, step 4) described in the low-temperature bake condition of post processing rear catalyst be: 200 ~ 300 DEG C, 2 ~ 4 hours.
The post processing hydrocracking catalyst that the inventive method prepares has the distribution of regulating catalyst surface metal levels, and then improves the feature of hydrocracking catalyst to high aromatic hydrocarbons hydrocarbon material inferior.Compared with prior art hydrogenation activity is higher, and hydrogenation selectivity is higher, thus selective higher to intermediate oil.And this kind of post-processing approach has versatility, be applicable to the hydrocracking catalyst of the various different metal composition of process.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Comparative example 1
(1) carrier preparation:
Get the adhesive that modified aluminas 50g, amorphous aluminum silicide 100g and USY molecular sieve 45g and 310g are made up of nitric acid and SB alumina peptization, kneading, rolls, and making can the paste of extrusion, extruded moulding.110 DEG C of dryings 6 hours, 550 DEG C of roastings 4 hours, obtained carrier A.
(2) catalyst preparing
Get 10g nickel nitrate, 29g ammonium metatungstate, be dissolved in the 70ml aqueous solution, then adopt equi-volume impregnating, W-Ni co-impregnated solution is immersed in 80g carrier A upper 2 hour, 110 DEG C of dryings 6 hours, 500 DEG C of roastings 2 hours, obtained catalyst catA.
Comparative example 2
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Get 7g basic nickel carbonate, 20g molybdenum trioxide, 4g phosphoric acid is dissolved in the 70ml aqueous solution, then adopt equi-volume impregnating, Mo-Ni-P co-impregnated solution is immersed in 80g carrier A upper 2 hour, 110 DEG C of dryings 6 hours, 500 DEG C of roastings 2 hours, obtained catalyst catB.
Embodiment 1
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Get 10g nickel nitrate, 29g ammonium metatungstate, be dissolved in the 70ml aqueous solution, then adopt equi-volume impregnating, W-Ni co-impregnated solution is immersed in 80g carrier A upper 2 hour, 110 DEG C of dryings 6 hours, 350 DEG C of roastings 2 hours, obtained catalyst catC.
(3) catalyst post processing
Get 2g tartaric acid to be dissolved in 15ml water, then constant volume is to 70ml, adopts equi-volume impregnating to be impregnated on 110g catalyst catC, dries in the shade after 2 hours, 100 DEG C of dryings 2 hours, and 250 DEG C of roastings 2 hours, obtain catD.
Embodiment 2
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Method is with the preparation method in Example 1
(3) catalyst post processing
Get 20g tartaric acid to be dissolved in 15ml water, then constant volume is to 70ml, adopts equi-volume impregnating to be impregnated on 110g catalyst catC, dries in the shade after 2 hours, 100 DEG C of dryings 2 hours, and 250 DEG C of roastings 2 hours, obtain catE.
Embodiment 3
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Method is with the preparation method in Example 1
(3) catalyst post processing
Get 60g tartaric acid to be dissolved in 15ml water, then constant volume is to 70ml, adopts equi-volume impregnating to be impregnated on 110g catalyst catC, dries in the shade after 2 hours, 100 DEG C of dryings 2 hours, and 250 DEG C of roastings 2 hours, obtain catF.
Embodiment 4
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Method is with the preparation method in Example 1.
(3) catalyst post processing
Get 20g tartaric acid to be dissolved in 15ml water, then constant volume is to 70ml, adopts equi-volume impregnating to be impregnated on 110g catalyst catC, dries in the shade after 2 hours, 100 DEG C of dryings 2 hours, and 350 DEG C of roastings 2 hours, obtain catH.
Embodiment 5
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Method is with the preparation method in Example 2.
(3) catalyst post processing
Get 40gATMP to be dissolved in 15ml water, then constant volume is to 70ml, adopts equi-volume impregnating to be impregnated on 110g catalyst catC, dries in the shade after 2 hours, 100 DEG C of dryings 2 hours, and 250 DEG C of roastings 2 hours, obtain catG.
Embodiment 6
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Method is with the preparation method in Example 2.
(3) catalyst post processing
Get 39.7gEDTA to be dissolved in 35ml ammoniacal liquor, then constant volume is to 70ml, adopts equi-volume impregnating to be impregnated on 110g catalyst catC, dries in the shade after 2 hours, 100 DEG C of dryings 2 hours, and 250 DEG C of roastings 2 hours, obtain catK.
Embodiment 7
(1) carrier preparation
Method is with the preparation method in comparative example 1.
(2) catalyst preparing
Get 7g basic nickel carbonate, 20g molybdenum trioxide, 4g phosphoric acid is dissolved in the 70ml aqueous solution, then adopt equi-volume impregnating, Mo-Ni-P co-impregnated solution is immersed in 80g carrier A upper 2 hour, 110 DEG C of dryings 6 hours, 350 DEG C of roastings 2 hours, obtained catalyst catL.
(3) catalyst post processing
Get 20g tartaric acid to be dissolved in 15ml water, then constant volume is to 70ml, adopts equi-volume impregnating to be impregnated on 110g catalyst catL, dries in the shade after 2 hours, 100 DEG C of dryings 2 hours, and 350 DEG C of roastings 2 hours, obtain catM.
Table 1 is the physical parameter of comparative example and embodiment catalyst.From data in table, the total acidity of the catalyst after complexing agent post processing obtains increase, is beneficial to the raising of hydrocracking catalyst cracking performance.
The different complexing agent content of table 1 and treatment temperature catalyst physical property
Table 1 is the impact of Different adding amount on hydrocracking catalyst, from data in table, along with the increase of complexing agent addition, specific area, pore volume, average pore size reduce gradually, but the total acid content of catalyst increases gradually, and this is conducive to the raising of hydrocracking catalyst cracking performance.
Table 2 different complexing agent kind post-processing catalyst physical property
| Catalyst is numbered | catE | catG | catK |
| Complexing agent kind | Tartaric acid | ATMP | EDTA |
| Complexing agent addition, g | 20 | 40 | 39.7 |
| With metal molar mass ratio | 1 | 1 | 1 |
| Post processing sintering temperature, DEG C | 250 | 250 | 250 |
| WO 3，wt％ | 22.3 | 22.3 | 22.3 |
| NiO，wt％ | 2.4 | 2.5 | 2.4 |
| Specific area, m 2/g | 260 | 253 | 249 |
| Pore volume, ml/g | 0.54 | 0.52 | 0.53 |
| Average pore diameter, nm | 5.68 | 5.58 | 5.71 |
| Infrared total acidity, mmol/g | 0.399 | 0.474 | 0.408 |
Table 2 is the impact of different complexing agent on catalyst performance, and from characterization result, when ensureing to remain unchanged with metal molar quality, different complexing agent all has increasing action to catalyst calculation amount, is beneficial to catalyst cracking performance and improves.
Table 3 different activities metallic catalyst physical property
| Catalyst is numbered | catA | catE | catM | CatB |
| Complexing agent kind | / | Tartaric acid | Tartaric acid | / |
| Complexing agent addition, g | / | 20 | 20 | / |
| With metal molar mass ratio | / | 1 | 1 | / |
| Post processing sintering temperature, DEG C | / | 250 | 250 | / |
| WO 3，wt％ | 22.2 | 22.3 | / | / |
| NiO，wt％ | 2.6 | 2.4 | 4.5 | 4.3 |
| M OO 3，wt％ | / | / | 20.1 | 20.3 |
| Specific area, m 2/g | 269 | 260 | 253 | 258 |
| Pore volume, ml/g | 0.56 | 0.54 | 0.52 | 0.55 |
| Average pore diameter, nm | 5.69 | 5.68 | 5.58 | 5.71 |
| Infrared total acidity, mmol/g | 0.267 | 0.399 | 0.474 | 0.232 |
Table 3 is the data of molybdenum nickel phosphorus system and nickel tungsten System Catalyst, there are data in table known, no matter be that the catalyst activity of which kind of system after post processing is all good than the structure of the catalyst through high-temperature roasting, and catalyst prepared by acid amount and conventional method want high a lot.
Table 4 is that catA and catE adopts SEM-EDS characterization result data, and can be found by data in table, the surface metal levels of post-processing catalyst is higher than conventional high temperature calcined catalyst really.
The different preparation method SEM-EDS characterization result of table 4
Can be found by data in table, the catalyst catA that the tenor that post processing type hydrocracking catalyst catE is positioned at catalyst surface is prepared apparently higher than conventional method.Appreciation condition: carry out on 200ml small hydrogenation device, raw materials used oil nature is in table 2.Operating condition is as follows: hydrogen dividing potential drop 14.7MPa, hydrogen to oil volume ratio 1500:1, volume space velocity 1.5h during liquid
-1.Catalyst Activating Test the results are shown in Table 5.
Table 5 feedstock oil character
| Feedstock oil title | Iran VGO |
| Density (20 DEG C), g/cm 3 | 0.9164 |
| Boiling range, DEG C | 528～531 |
| Viscosity (50 DEG C), mm 2/s | 33.69 |
| Viscosity (100 DEG C), mm 2/s | 6.944 |
| Condensation point, DEG C | 34 |
| Acid number, mgKOH/g | 0.49 |
| Carbon residue, wt% | 0.32 |
| S，μg/g | 16000 |
| N，μg/g | 1475 |
| C，wt％ | 85.25 |
| H，wt％ | 11.96 |
| BMCI value | 48.2 |
| Refractive power/n D 70 | 1.4899 |
Table 6 evaluating catalyst result
| Catalyst is numbered | catA | catD | catE | catF | CatH |
| Reaction temperature, DEG C | 385 | 385 | 385 | 385 | 385 |
| Middle distillates oil selectivity, % | 80.6 | 82.8. | 85.3 | 80.1 | 84.2 |
| Jet fuel yield wt% | 27.6 | 28.9 | 30.5 | 29.1 | 29.6 |
| Diesel yield, wt% | 17.3 | 18.6 | 19.9 | 18.4 | 19.0 |
Can be found by data in table 6 and adopt compared with the catA after high-temperature roasting, the yield that physical property and jet fuel and diesel oil are selected in the middle grease separation of post processing type catalyst is all higher, and along with the increase of complexing agent content, actively occurs an optimum value.Contrast catE and catH finds, higher post-processing temperature is unfavorable to catalyst properties.
Table 7 evaluating catalyst result
| Catalyst is numbered | catG | catK | catA | catE | catM | CatB |
| Reaction temperature, DEG C | 385 | 385 | 385 | 385 | 385 | 385 |
| Middle distillates oil selectivity, % | 86.2 | 83.8 | 80.6 | 85.3 | 84.7 | 80.6 |
| Jet fuel yield wt% | 31.6 | 29.9 | 27.6 | 30.5 | 29.6 | 26.7 |
| Diesel yield, wt% | 19.8 | 18.6 | 17.3 | 19.9 | 18.0 | 19.8 |
Can be found by data in table 7, catalyst catG, catK, catE after different complexing agent post processing are good than the catalyst catA after high-temperature roasting at various aspect of performance.And adopt the post-processing catalyst performance of organic phosphine acids to be more suitable for processing inferior raw material.Also there is the experimental result similar to nickel tungsten system in catalyst CatB and the CatM adopting molybdenum nickel phosphorus system to prepare, post processing type catalyst is better than the catalyst of high-temperature roasting, illustrates that this kind of method has general applicability.
Claims (6)
1. a preparation method for post processing type hydrocracking catalyst, is characterized in that:
1) carrier of hydrocracking catalyst is prepared;
2) adopt equi-volume impregnating to be impregnated in catalyst carrier the maceration extract containing active metal component, then dry, at 200 ~ 400 DEG C low-temperature bake 1 ~ 10 hour.
3) step 2 is impregnated into after the material that can change active metal arrangement is by a certain percentage dissolved in solvent) catalyst that obtains;
4) step 3) material that obtains carries out drying, be within 1 ~ 10 hour, obtain final post processing type hydrocracking catalyst 150 ~ 400 DEG C of low-temperature bake times;
Wherein, step 3) described in the material that can change active metal arrangement be one or more in phosphoric acid class, alcamines, aminocarboxylic acids, hydroxycarboxylic acid, organic phosphine acids, polyacrylic complexing agent;
Described can change active metal arrangement material addition and catalyst in the mol ratio of active metal component be 0.1 ~ 5.
2., according to preparation method according to claim 1, it is characterized in that, step 2) described in low-temperature bake condition be: roasting 1 ~ 3 hour at 300 ~ 400 DEG C.
3. according to preparation method according to claim 1, it is characterized in that, described phosphoric acid class is one or more in tripolyphosphate, pyrophosphoric acid and hexa metaphosphoric acid; Alcamines is one or more in MEA, diethanol amine and triethanolamine; Aminocarboxylic acids is one or more in nitrilotriacetic acid, ethylenediamine tetra-acetic acid, diethylenetriamine pentacarboxylic acid; Hydroxycarboxylic acid is one or more in tartaric acid, heptonic acid, gluconic acid, alginic acid; Organic phosphine acids is one or more in ATMP, HEDP, ethylenediamine tetraacetic methene phosphoric acid, diethylene triamine pentamethylene phosphonic and amine three methene phosphoric acid; Polyacrylic is one or more in HPMA, polyacrylic acid, poly-hydroxy acrylic acid, maleic acrylic copolymer and polyacrylamide.
4. according to preparation method according to claim 1, it is characterized in that, the described material that can change active metal arrangement is hydroxycarboxylic acid complexing agent or organic phosphine acids complexing agent.
5., according to preparation method according to claim 1, it is characterized in that, described can change active metal arrangement material addition and catalyst in the mol ratio of active metal component be 0.1 ~ 3.
6., according to preparation method according to claim 1, it is characterized in that, step 4) described in the low-temperature bake condition of post processing rear catalyst be: 200 ~ 300 DEG C, 2 ~ 4 hours.
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| CN110038623A (en) * | 2018-01-16 | 2019-07-23 | 中国石油化工股份有限公司 | Hydrocracking catalyst and preparation method thereof |
| CN110038618B (en) * | 2018-01-16 | 2021-12-07 | 中国石油化工股份有限公司 | Preparation method of hydrocracking catalyst |
| CN110038622B (en) * | 2018-01-16 | 2021-12-07 | 中国石油化工股份有限公司 | Hydrocracking catalyst and preparation method thereof |
| CN111097433A (en) * | 2018-10-26 | 2020-05-05 | 中国石油化工股份有限公司 | Regeneration method of deactivated residual oil hydrotreating catalyst |
| CN112705212A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Regeneration method of deactivated residual oil hydrotreating catalyst |
| CN112705212B (en) * | 2019-10-25 | 2023-10-10 | 中国石油化工股份有限公司 | Regeneration method of deactivated residuum hydrotreatment catalyst |
| CN113509954A (en) * | 2020-04-09 | 2021-10-19 | 中国石油化工股份有限公司 | Preparation method and application of passivated sulfuration-state hydrocracking catalyst |
| CN114917939A (en) * | 2022-05-05 | 2022-08-19 | 山东公泉化工股份有限公司 | Preparation method of catalyst impregnation liquid |
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